CN104843713B - A kind of pyrolytic prodan prepares method and the device thereof of Silicon fluoride. - Google Patents
A kind of pyrolytic prodan prepares method and the device thereof of Silicon fluoride. Download PDFInfo
- Publication number
- CN104843713B CN104843713B CN201510302232.7A CN201510302232A CN104843713B CN 104843713 B CN104843713 B CN 104843713B CN 201510302232 A CN201510302232 A CN 201510302232A CN 104843713 B CN104843713 B CN 104843713B
- Authority
- CN
- China
- Prior art keywords
- flanging
- prodan
- kettle
- central authorities
- pallet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of pyrolytic prodan and prepare method and the device thereof of Silicon fluoride., prodan first carries out washing purify, it is then charged into decomposition reaction still heat resolve in the way of thin layer, static state, collects and obtain collecting after silicon tetrafluoride gas is condensed by heat exchanger.Having tray rack in the kettle of special decomposition reaction still, tray rack can be put multiple heating pallet, heating pallet is annulus shape, and heating pallet has on surrounding flanging and central authorities' flanging, surrounding flanging and central authorities' flanging and has ventilation breach；Surrounding flanging and inner wall of kettle form gas outlet channels, also form center gas outlet duct between central authorities' flanging；Blind flange is connected with kettle by connecting bolt and packing ring, and blind flange top connects escape pipe.The inventive method uses a point dish, static mode heat resolve prodan to prepare silicon tetrafluoride gas, has that apparatus structure is simple, requirement of strength is low, the advantage easily preparing high-purity silicon tetrafluoride gas.
Description
Technical field
The invention belongs to chemical machinery field, be specifically related to a kind of high temperature thermal decomposition and prepare method and the device thereof of silicon tetrafluoride gas.
Background technology
Silicon fluoride. is a kind of important source material in electronics and semicon industry, is mainly used in the etchant of tantalum silicide, silicon nitride etc., P-type dopant and epitaxial deposition diffusion silicon source, it is also possible to be used for preparing electronic-grade silane or polysilicon；Owing to Silicon fluoride. hydrolyzes to produce in thermal-flame, there is the heat sink SiO of high-specific surface area2, it is also possible to it is used for making optical fibers pure quartz glass；In optical fiber production technology, the important component of the ion implantation that Silicon fluoride. is used when being and manufacture silicon-based semiconductor devices；Additionally, Silicon fluoride. is also widely used for producing cement, electronic material, solar cell device, photocopier photosensitive drums, ULSI etc., the development applied along with laser, it is also possible to as photosensitizer etc. in organic reaction.
The preparation method that silicon tetrafluoride gas is conventional, including sulfuric acid process, hydrogen fluoride, Si-F2Direct synthesis technique and fluosilicate pyrolysismethod etc..Wherein in addition to fluosilicate pyrolysismethod, other preparation method is required to introduce acid or fluorine gas, and the subsequent purification for Silicon fluoride. increases difficulty.And fluosilicate pyrolysismethod is without introducing other reactant, reaction is prone to occur, and operational danger is little, requires also low than sulfuric acid process and hexafluosilicic acid method to equipment material.Fluosilicate can first pass through purification in advance, and the silicon tetrafluoride gas that pyrolysis obtains is also easy to purify further, and side-product fluoride salt is also the important raw material of industry, and therefore the method becomes the method preparing electron level silicon tetrafluoride gas that is more conventional and that have development prospect.Phosphate fertilizer by-product product prodan yield is big, price is low, therefore becomes the raw material that thermal decomposition preparation silicon tetrafluoride gas is the most commonly used.
But prodan easily occurs vitreous clinker to cause decomposing difficulty in heating process.Solution generally uses interpolation precipitation additive, or reaction unit is designed as using fluid bed or the pattern of rotary kiln, indeed through being stirred prodan avoiding alleviating Caking Tendency.
In Chinese patent storehouse, the application part relevant to prodan high temperature decomposition device has: 200980156839.1 " for being produced method and the system of Silicon fluoride. in a fluidized bed reactor by fluosilicate ", 201110258173.X " using the method that Silicon fluoride. prepared by rotary kiln ", 200910024293.6 " methods of preparing silicon tetrafluoride through pyrolysis of sodium fluosilicate in rotary reaction furnace ".Above-mentioned patented technology all can prepare silicon tetrafluoride gas by pyrolytic fluosilicate, but high to equipment corrosion resistance and requirement of strength；Additionally, use the mode (fluid bed or rotary kiln) of fluosilicate dynamic Decomposition to prepare Silicon fluoride., a large amount of material dust can be produced in process of production, increase Silicon fluoride. subsequent purification difficulty, and caking phenomenon can not be avoided completely.
Summary of the invention
It is an object of the invention to provide a kind of pyrolytic prodan and prepare method and the device thereof of silicon tetrafluoride gas, the method and device improve Fluoride for Raw Material sodium silicate thermolytic rate, largely improve it and decompose caking phenomenon, material dust will not be produced, thus reduce Silicon fluoride. subsequent purification and purify difficulty.
The purpose of the present invention and solve its technical problem underlying and realize by the following technical solutions: a kind of method that pyrolytic prodan prepares Silicon fluoride., it is characterized in that: first prodan is carried out washing and purifies, reduce and decompose the impurity obtaining in silicon tetrafluoride gas, it is then charged into special decomposition reaction still heat resolve in the way of thin layer, static state, collects after the silicon tetrafluoride gas obtained is condensed by heat exchanger and collect；Specifically comprise the following steps that
(1) method that prodan washing purifies is that wash temperature is 10 DEG C～100 DEG C, and institute's water consumption is 3 times～10 times of prodan quality；Washing methods is to be mixed with water by prodan, and then stirring 5min～30min, then filters, and filter cake is dried 1-3 hour at 100 DEG C～300 DEG C, is down to room temperature in being subsequently placed in exsiccator；
(2) will contain in multiple heating pallets of special decomposition reaction still after the prodan of washing is mixed homogeneously with precipitation additive, loading height be 1mm～20mm and less than the ventilation breach on pallet；Then being stacked by heating pallet and be placed in decomposing in kettle to tray rack, heating-up temperature is 500 DEG C～900 DEG C.
Described precipitation additive is sodium fluoride.
Described special decomposition reaction still, including kettle and blind flange, has tray rack in kettle, tray rack can be put multiple heating pallet, and heating pallet is annulus shape, and heating pallet has on surrounding flanging and central authorities' flanging, surrounding flanging and central authorities' flanging and has ventilation breach；Surrounding flanging and inner wall of kettle form gas outlet channels, also form center gas outlet duct between central authorities' flanging；Blind flange top connects escape pipe.
Further, blind flange is connected with kettle by connecting bolt and packing ring.
During use, prodan after washing being purified loads in heating pallet, then heating pallet is stacked to tray rack and put in decomposition kettle, build blind flange, it is placed in heating furnace heating and obtains silicon tetrafluoride gas, discharge from escape pipe through gas outlet channels and center gas outlet duct, collect after being condensed by heat exchanger.
The present invention compared with prior art has clear advantage and beneficial effect.From above technical scheme, first the present invention carries out washing and purifies prodan, reduces the impurity silicon tetrafluoride gas from source.And have employed multiple layer tray first and decompose the mode of prodan, raw thickness is reduced, improves Fluoride for Raw Material sodium silicate thermolytic rate, and largely improve it and decompose caking phenomenon；In heating process, prodan and precipitation additive are in static state, will not produce material dust, thus reduce Silicon fluoride. subsequent purification and purify difficulty；Use tray rack fixing heating pallet, it is ensured that decomposition reaction still is transported pallet during the course and is difficult to topple, it is ensured that silicon tetrafluoride gas passing away is unobstructed.
Accompanying drawing explanation
Fig. 1 is the structural representation that pyrolytic prodan of the present invention prepares Silicon fluoride. device,
Fig. 2 is the top view of Fig. 1,
Fig. 3 is the heating support holder structure schematic diagram of the present invention,
Fig. 4 is that the pallet charging of the present invention stacks schematic diagram.
Labelling in figure: 1, blind flange, 2, escape pipe, 3, kettle, 4, tray rack, 5, heating pallet, 6, surrounding flanging, 7, central authorities' flanging, 8, ventilation breach, 9, packing ring, 10, connecting bolt, 11, gas outlet channels, 12, center gas outlet duct.
Detailed description of the invention
Below in conjunction with accompanying drawing and preferred embodiment, method and device detailed description of the invention, feature and effect thereof of Silicon fluoride. are prepared by a kind of pyrolytic prodan proposed according to the present invention, after describing in detail such as.
See Fig. 1-4, a kind of method that pyrolytic prodan prepares silicon tetrafluoride gas, it is characterized in that: first prodan is carried out washing and purifies, reduce and decompose the impurity obtaining in silicon tetrafluoride gas, it is then charged into special decomposition reaction still heat resolve in the way of thin layer, static state, collects after the silicon tetrafluoride gas obtained is condensed by heat exchanger and collect；Specifically comprise the following steps that
(1) method that prodan washing purifies is that wash temperature is 10 DEG C～100 DEG C, and institute's water consumption is 3 times～10 times of prodan quality；Washing methods is to be mixed with water by prodan, and then stirring 5min～30min, then filters, and filter cake is dried 1-3 hour at 100 DEG C～300 DEG C, is down to room temperature in being subsequently placed in exsiccator；
(2) will contain in multiple heating pallets of special decomposition reaction still after the prodan of washing is mixed homogeneously with precipitation additive, loading height be 1mm～20mm and less than the ventilation breach on pallet；Then being stacked by heating pallet and be placed in decomposing in kettle to tray rack, heating-up temperature is 500 DEG C～900 DEG C.
Described precipitation additive is sodium fluoride.
Described special decomposition reaction still, including kettle 3 and blind flange 1, has tray rack 4 in kettle 3, multiple heating pallet 5 can be put on tray rack 4, heating pallet 5 is in annulus shape, and heating pallet 5 has on surrounding flanging 6 and central authorities' flanging 7, surrounding flanging 6 and central authorities' flanging 7 and has ventilation breach 8；Surrounding flanging 6 and kettle 3 inwall form gas outlet channels 11, also form center gas outlet duct 12 between central authorities' flanging 7；Blind flange 1 top connects escape pipe 2.
Further, blind flange 1 is connected with kettle 3 by connecting bolt 10 and packing ring 9,
During use, prodan after washing being purified loads in heating pallet 5, then heating pallet 5 is stacked to tray rack 4 and put in decomposition kettle 3, build blind flange 1, it is placed in heating furnace heating and obtains silicon tetrafluoride gas, discharge from escape pipe 2 through gas outlet channels 11 and center gas outlet duct 12, collect after being condensed by heat exchanger.
Embodiment: prodan carrying out washing and purifies, water consumption is 10 times of water yields of prodan quality, and wash temperature is 95 DEG C, wash time is 30min.Then filtering, filter cake is vacuum dried 1 hour at 200 DEG C；Mixing homogeneously with precipitation additive afterwards, be then charged into heating pallet, height is 10mm and less than the ventilation breach on flanging；Then heating pallet is stacked to tray rack, proceed in kettle afterwards；Then place packing ring, top flange dish, tighten connecting bolt；Afterwards, being placed in shaft furnace heating, heating-up temperature is 750 DEG C, decomposes the silicon tetrafluoride gas produced and collects after heat exchanger is lowered the temperature.
The mode that the present invention uses point dish thin layer to decompose avoids prodan vitreous clinker, improves and decomposes productivity；The mode using static heat resolve avoids material dust to produce, thus more conducively silicon tetrafluoride gas subsequent purification purifies.
The above, it it is only presently preferred embodiments of the present invention, not the present invention is made any pro forma restriction, any without departing from technical solution of the present invention content, any simple modification, equivalent variations and the modification made above example according to the technical spirit of the present invention, all still falls within the range of technical solution of the present invention.
Claims (3)
1. the method that a pyrolytic prodan prepares Silicon fluoride., it is characterized in that: first prodan is carried out washing and purifies, reduce and decompose the impurity obtaining in silicon tetrafluoride gas, it is then charged into special decomposition reaction still heat resolve in the way of thin layer, static state, collects after the silicon tetrafluoride gas obtained is condensed by heat exchanger and collect；Specifically comprise the following steps that
(1) method that prodan washing purifies is that wash temperature is 10 DEG C～100 DEG C, and institute's water consumption is 3 times～10 times of prodan quality；Washing methods is to be mixed with water by prodan, and then stirring 5min～30min, then filters, and filter cake is dried 1-3 hour at 100 DEG C～300 DEG C, is down to room temperature in being subsequently placed in exsiccator；
(2) will contain in multiple heating pallets of special decomposition reaction still after the prodan of washing is mixed homogeneously with precipitation additive, loading height be 1mm～20mm and less than the ventilation breach on pallet；Then being stacked by heating pallet and be placed in decomposing heat resolve in kettle to tray rack, heating-up temperature is 500 DEG C～900 DEG C；
Described precipitation additive is sodium fluoride；
Described special decomposition reaction still, including kettle (3) and blind flange (1), tray rack (4) is had in kettle (3), multiple heating pallet (5) is put on tray rack (4), heating pallet (5) is in annulus shape, heating pallet (5) has in surrounding flanging (6) and central authorities' flanging (7), surrounding flanging (6) and central authorities' flanging (7) and has ventilation breach (8)；Surrounding flanging (6) and kettle (3) inwall form gas outlet channels (11), also form center gas outlet duct (12) between central authorities' flanging (7)；Blind flange (1) top connects escape pipe (2).
A kind of pyrolytic prodan the most as claimed in claim 1 prepares the device used by method of Silicon fluoride., it is characterized in that: include kettle (3) and blind flange (1), tray rack (4) is had in kettle (3), multiple heating pallet (5) is put on tray rack (4), heating pallet (5) is in annulus shape, heating pallet (5) has in surrounding flanging (6) and central authorities' flanging (7), surrounding flanging (6) and central authorities' flanging (7) and has ventilation breach (8)；Surrounding flanging (6) and kettle (3) inwall form gas outlet channels (11), also form center gas outlet duct (12) between central authorities' flanging (7)；Blind flange (1) top connects escape pipe (2).
A kind of pyrolytic prodan the most as claimed in claim 2 prepares the device used by method of Silicon fluoride., it is characterised in that: blind flange (1) is connected with kettle (3) by connecting bolt (10) and packing ring (9).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510302232.7A CN104843713B (en) | 2015-06-04 | 2015-06-04 | A kind of pyrolytic prodan prepares method and the device thereof of Silicon fluoride. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510302232.7A CN104843713B (en) | 2015-06-04 | 2015-06-04 | A kind of pyrolytic prodan prepares method and the device thereof of Silicon fluoride. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104843713A CN104843713A (en) | 2015-08-19 |
| CN104843713B true CN104843713B (en) | 2016-10-12 |
Family
ID=53843764
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510302232.7A Expired - Fee Related CN104843713B (en) | 2015-06-04 | 2015-06-04 | A kind of pyrolytic prodan prepares method and the device thereof of Silicon fluoride. |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104843713B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112441604B (en) * | 2019-08-28 | 2022-08-12 | 多氟多新材料股份有限公司 | Method for preparing high-purity fluoride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698482A (en) * | 2009-10-13 | 2010-04-28 | 西安三瑞实业有限公司 | Method for preparing silicon tetrafluoride through pyrolysis of sodium fluosilicate in rotary reaction furnace |
| CN101812085A (en) * | 2010-03-22 | 2010-08-25 | 云南省化工研究院 | Method for producing tetraethoxy-silicone and anhydrous hydrogen fluoride from sodium fluosilicate |
| CN102398906A (en) * | 2011-07-22 | 2012-04-04 | 多氟多化工股份有限公司 | Method for producing SiF4 from Na2SiF6 through pyrolysis |
| CN204643859U (en) * | 2015-06-04 | 2015-09-16 | 贵州省产品质量监督检验院 | A kind of pyrolytic decomposition Sodium Silicofluoride prepares the device of silicon tetrafluoride |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6374910A (en) * | 1986-09-19 | 1988-04-05 | Mitsui Toatsu Chem Inc | Production of high-purity silicon tetrafluoride |
-
2015
- 2015-06-04 CN CN201510302232.7A patent/CN104843713B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698482A (en) * | 2009-10-13 | 2010-04-28 | 西安三瑞实业有限公司 | Method for preparing silicon tetrafluoride through pyrolysis of sodium fluosilicate in rotary reaction furnace |
| CN101812085A (en) * | 2010-03-22 | 2010-08-25 | 云南省化工研究院 | Method for producing tetraethoxy-silicone and anhydrous hydrogen fluoride from sodium fluosilicate |
| CN102398906A (en) * | 2011-07-22 | 2012-04-04 | 多氟多化工股份有限公司 | Method for producing SiF4 from Na2SiF6 through pyrolysis |
| CN204643859U (en) * | 2015-06-04 | 2015-09-16 | 贵州省产品质量监督检验院 | A kind of pyrolytic decomposition Sodium Silicofluoride prepares the device of silicon tetrafluoride |
Non-Patent Citations (1)
| Title |
|---|
| 四氟化硅的工艺研发及进展状况;韩建军等;《无机盐工业》;20130131;第45卷(第1期);第4-7页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104843713A (en) | 2015-08-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2070871B1 (en) | Process for production of multicrystal silicon and facility for production of multicrystal silicon | |
| CN101279735A (en) | Production method and apparatus for trichlorosilane | |
| CN102030329B (en) | Polycrystalline silicon producing device and process | |
| CN102674358B (en) | Method for preparing polysilicon and system | |
| CN101544374B (en) | Method for preparing silicon tetrafluoride | |
| CN104843713B (en) | A kind of pyrolytic prodan prepares method and the device thereof of Silicon fluoride. | |
| CN102398906A (en) | Method for producing SiF4 from Na2SiF6 through pyrolysis | |
| CN204643859U (en) | A kind of pyrolytic decomposition Sodium Silicofluoride prepares the device of silicon tetrafluoride | |
| CN102786055A (en) | Method and device for heat utilization in polycrystalline silicon production process | |
| CN101928002A (en) | Method for producing polysilicon with silicon tetrafluoride reduced by plasmas | |
| CN102674368A (en) | Method and system for preparing trichlorosilane | |
| CN112441604B (en) | Method for preparing high-purity fluoride | |
| CN202072477U (en) | Polycrystalline silicon production system | |
| CN101723370B (en) | Polysilicon production method without silicon tetrachloride emission | |
| CN103172067B (en) | Cold wall fluidized bed and application thereof | |
| CN106115718B (en) | A kind of disilane process units | |
| CN104556054A (en) | Method and device for recycling light components in trichlorosilane synthetic compost | |
| CN104891499A (en) | Technological method for preparing polysilicon by silane method | |
| CN208454506U (en) | A kind of monosilane thermal decomposition furnace of truncated cone-shaped cooling jacket | |
| CN209242693U (en) | Purify the device of trichlorosilane | |
| CN101880044A (en) | Method for preparing solar grade silicon by disproportionation reaction | |
| CN103626184B (en) | A kind of preparation method of high-purity liquid polysilicon | |
| CN112158849A (en) | Method for preparing silicon tetrafluoride from phosphorus ore associated fluorine | |
| CN214880244U (en) | Novel production device for synthesizing trichlorosilane | |
| CN209835648U (en) | Purification device of raw material silicon source for producing high-purity silicon carbide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161012 Termination date: 20200604 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |